CN108409984A - A kind of method that Fast synchronization prepares lignin nanoparticle and carbon quantum dot - Google Patents
A kind of method that Fast synchronization prepares lignin nanoparticle and carbon quantum dot Download PDFInfo
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- CN108409984A CN108409984A CN201810250553.0A CN201810250553A CN108409984A CN 108409984 A CN108409984 A CN 108409984A CN 201810250553 A CN201810250553 A CN 201810250553A CN 108409984 A CN108409984 A CN 108409984A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The invention discloses a kind of methods that Fast synchronization prepares lignin nanoparticle and carbon quantum dot, are as follows：Abandoned biomass is added in acid solution, is separated by solid-liquid separation after microwave treatment and obtains treatment fluid；Treatment fluid is centrifuged, gained lower sediment is lignin nanoparticle, and gained supernatant liquor is nitrogen-doped carbon quantum dot solution, and the solvent in the acid solution is the mixed solvent comprising ethyl alcohol.This method can prepare the biomass nano material of different scale using abandoned biomass Fast synchronization, including lignin nanoparticle (~100nm) and fluorescence nitrogen-doped carbon quantum dot (2 3nm), the universality of Conventional nano material preparation method is greatly improved.And the preparation method that the invention is related to is quick, green, simple, is easy to industrialized production, it is of low cost.
Description
Technical field：
The invention belongs to biomass nano technical field of material chemistry, and in particular to a kind of Fast synchronization prepares lignin nanometer
The method of grain and carbon quantum dot.
Background technology：
Function c-based nanomaterial because its with unique tunable characteristic (for example, heat and electric conductivity, high mechanical properties and light
Learn performance), it is the key that solve environment and energy crisis.At this stage, ever-increasing industrial requirement have stimulated to it is nontoxic, low at
The research of this and environmentally friendly preparation method.Active ingredient of the lignocellulosic as agriculture and forestry organic waste material is most rich on the earth
Rich, most cheap renewable resource, biocompatibility and biological degradability make its including biomedical devices, electronics and
Change technical field including the energy has huge application potential.Therefore, the nano meter biomaterial prepared by lignocellulosic
Becoming a kind of very attractive solution.
Recent study finds that lignin nano-particle can prepare function by the way that function to be introduced into polymeric matrix
Property polymer composite, to substitute toxic nano material.In view of its good property, the functional nanocomposite is in medicine
Object transport system provides hydrophobic molecule, has valued added applications in terms of enhancing ultraviolet light barrier, antibacterial and antioxygenic property.It is general and
Speech, preparing uniform lignin nanoparticle, mainly lignin liquor is passed through control by (drop fills or dialysis) in a controlled manner
System precipitation realizes the preparation of particle, i.e. micelle formation.In addition, another zero dimension (~10nm) carbon family nano material carbon quantum
Point also results in very big pass due to its optical property and its application in terms of bio-imaging, drug delivery and biosensor
Note.Studies have shown that carbon quantum dot can also utilize abandoned biomass to prepare.Although having some at present about lignin nanoparticle
The report prepared with carbon quantum dot, but big multi-method is related to that complicated process and exacting terms, grain size is difficult to control, time-consuming
(for up to 3 days) are expensive, and therefore, it is difficult to promote and apply.
Invention content：
In view of the deficiencies of the prior art, the present invention is intended to provide a kind of Fast synchronization prepares lignin nanoparticle and carbon amounts
The method of son point, this method is easy to operate, it is extremely short, at low cost to take, and can realize lignin nanoparticle and carbon quantum dot
Synchronization one kettle way prepare, realize the functional material recycling of abandoned biomass.
To achieve the above object, the present invention provides the following technical solutions：
Abandoned biomass is added in acid solution, is separated by solid-liquid separation after microwave treatment and obtains treatment fluid；To treatment fluid centrifugation point
From gained lower sediment is lignin nanoparticle, and gained supernatant liquor is nitrogen-doped carbon quantum dot solution；
Solvent in the acid solution is the mixed solvent comprising ethyl alcohol；
The acid is non-oxidizing acid；
H in the acid solution+A concentration of 0.13mol/L~0.27mol/L.
In acid does the heat treatment of catalyst, the lignin in abandoned biomass is more than itself fusing point, is moved from cell wall
It is shifted out.Lignin is that have amphiphilic block copolymer, after being detached with lignocellulosic, hydrophobicity one end when being contacted with water
Micella core is formed, while hydrophily one end forms micelle shell, to form the blank of lignin nanoparticle.In aqueous solution,
Its particle formed is deposited on abandoned biomass surface at once, and the present invention utilizes the mixed solution containing ethyl alcohol, molten by changing
The polarity of liquid so that the particle of formation will not deposit at once, and be suspended in solution.The particle of suspension gradually form it is spherical with
Reduce its surface energy.
The solid-liquid mass volume ratio of preferred scheme, the abandoned biomass and acid solution is 1:10-1:20(g/ml).Make
To be further preferred, the solid-liquid mass volume ratio of the abandoned biomass and acid solution is 1:10-1:15(g/ml).As more into
One step is preferred, and the solid-liquid mass ratio of the abandoned biomass and acid solution is 1:10(g/ml).
Preferred scheme, the acid solution refer to the mixed solution dissolved with HCl.
Inventor has found that influence of the sour concentration to lignin nanoparticle is very big, and concentration is too small under study for action, will be unable to
Catalytic action is played, lignin nanoparticle can not be prepared.Concentration is excessive, and the size of gained lignin nanoparticle will become
Greatly, and it is uneven, and lose nano effect.
Preferred scheme, mass fractions of the HCl in acid solution are 0.5%-1%.
As a further preference, mass fractions of the HCl in acid solution is 0.5%-0.8%.
Preferred scheme, the mixed solvent are made of second alcohol and water.
The volume ratio of preferred scheme, the in the mixed solvent, second alcohol and water is 50:50-80:20.Preferably, described
The volume ratio of in the mixed solvent, second alcohol and water is 60:40-70:30.As further preferred, the in the mixed solvent, second
The volume ratio of alcohol and water is 60:40-65:35.
Preferred scheme, the abandoned biomass are selected from rice straw, maize straw, wheat stalk, bagasse, withy
At least one of millet.
Preferred scheme, the mesh of the grain size of the abandoned biomass≤60.
Preferred scheme, the abandoned biomass first after being crushed to above-mentioned grain size, then through ultra-pure water cleaning, be dried to perseverance
Weight.As a further preference, the Wen Weiwei 40-80 DEG C of the drying.
The power of preferred scheme, microwave treatment is 400-500W, and the time of microwave treatment is 7-15min.In the present invention
In, the time of the microwave treatment refers in setting power, and microwave equipment starts the time closed to microwave equipment.
The rotating speed of preferred scheme, the centrifugation is 10000-14000rpm, time 5-10min.
The average grain diameter of technical solution of the present invention, gained lignin nanoparticle is 123~187nm, gained nitrogen-doped carbon
The grain size of quantum dot is 2-3nm.
The advantage of preprocess method provided by the invention is：
(1) for the present invention using abandoned biomass, that is, lignocellulosic as raw material is prepared, source is wide, at low cost, is related to
Reagent is pollution-free, cheap, has and promotes and applies potentiality.
(2) preparation method of the present invention is quick, and green, easy to operate, equipment requirement is low, is especially taking aspect,
The present invention only needs that the preparation from raw material to finished product can be completed within 30min.
(3) lignin nanoparticle that the present invention prepares has nanometer size effect, and particle diameter distribution is uniform, dispersibility
Height, thermal stability is good, improves the potential application range of lignin.
(4) the nitrogen-doped carbon quantum dot that the present invention prepares has up-conversion fluorescence effect, and particle diameter distribution is uniform.
(5) method provided by the invention can synchronize the function carbon nanomaterial for preparing different scale, substantially increase
The preparation efficiency of function carbon nanomaterial.
Description of the drawings:
Fig. 1：Lignin nanoparticle scanning electron microscopic picture prepared by the present invention；
Fig. 2：Lignin nanoparticle Fourier's IR Characterization figure prepared by the present invention；
Fig. 3：Nitrogen-doped carbon quantum dot transmission electron microscope picture prepared by the present invention；
Fig. 4：Nitrogen-doped carbon quantum dot X-ray diffraction phenogram prepared by the present invention.
Specific implementation mode
Present invention is further described in detail in the following with reference to the drawings and specific embodiments, but not as the limit to the present invention
It is fixed.
Embodiment 1
(1) 60 mesh are sieved after crushing rice straw, and ultra-pure water cleans twice, and drying to constant weight in 60 DEG C.
(2) will through step (1), treated, and rice straw is placed in counteracting tank, by solid-to-liquid ratio be 1:10 (g/ml) are added molten
Solution has the alcohol-water (ethyl alcohol of HCl：Water is 65:35, v/v) it in mixed solution, is then allowed to stand in micro-wave oven (Glanz
P70F20L-DG in), after 400W microwave treatments 10min, treatment fluid, quality of the HCl in mixed solution is obtained by filtration
Score is 0.5%.
(3) the treatment fluid 12000rpm of acquisition is centrifuged into 10min, gained sediment is lignin nanoparticle, and upper layer is clear
Liquid is nitrogen-doped carbon quantum dot solution.
The average grain diameter of the lignin nanoparticle (such as Fig. 1) of preparation through this embodiment is 123nm, and particle diameter distribution
More uniformly (coefficient of dispersion is：0.173, such as Fig. 2), there is typical polyhydroxy lignin structure (such as Fig. 3).It prepares simultaneously
Nitrogen-doped carbon quantum point grain diameter be that (as shown in figure 4, carbon and oxygen are main peak, lower nitrogen peak shows that the quantum dot has nitrogen to 2-3nm
Doping), there is significant up conversion property.
Embodiment 2
(1) 60 mesh are sieved after crushing rice straw, and ultra-pure water cleans twice, and drying to constant weight in 60 DEG C.
(2) will through step (1), treated, and rice straw is placed in counteracting tank, by solid-to-liquid ratio be 1:15 (g/ml) are added molten
Solution has the alcohol-water (ethyl alcohol of HCl：Water is 60:40, v/v) it in mixed solution, is then allowed to stand in micro-wave oven (Glanz
P70F20L-DG in), after 500W microwave treatments 8min, treatment fluid, quality of the HCl in mixed solution point is obtained by filtration
Number is 0.5%.
(3) the treatment fluid 14000rpm of acquisition is centrifuged into 5min, gained sediment is lignin nanoparticle, supernatant liquor
For nitrogen-doped carbon quantum dot solution.
The average grain diameter of the lignin nanoparticle of preparation through this embodiment is that (coefficient of dispersion is 156nm：
0.201), there is typical polyhydroxy lignin structure.The nitrogen-doped carbon quantum point grain diameter prepared simultaneously is 2-3nm, is had
Significant up conversion property.
Embodiment 3
(1) 60 mesh are sieved after crushing rice straw, and ultra-pure water cleans twice, and drying to constant weight in 60 DEG C.
(2) will through step (1), treated, and rice straw is placed in counteracting tank, by solid-to-liquid ratio be 1:20 (g/ml) are added molten
Solution has the alcohol-water (ethyl alcohol of HCl：Water is 70:30, v/v) it in mixed solution, is then allowed to stand in micro-wave oven (Glanz
P70F20L-DG in), after 400W microwave treatments 12min, treatment fluid, quality of the HCl in mixed solution is obtained by filtration
Score is 0.8%.
(3) the treatment fluid 11000rpm of acquisition is centrifuged into 10min, gained sediment is lignin nanoparticle, and upper layer is clear
Liquid is nitrogen-doped carbon quantum dot solution.
The average grain diameter of the lignin nanoparticle of preparation through this embodiment is that (coefficient of dispersion is 187nm：
0.165), there is typical polyhydroxy lignin structure.The nitrogen-doped carbon quantum point grain diameter prepared simultaneously is 2-3nm, is had
Significant up conversion property.
Comparative example 1
(1) 60 mesh are sieved after crushing rice straw, and ultra-pure water cleans twice, and drying to constant weight in 60 DEG C.
(2) will through step (1), treated, and rice straw is placed in counteracting tank, by solid-to-liquid ratio be 1:10 (g/ml) are added molten
Solution has the alcohol-water (ethyl alcohol of HCl：Water is 65:35, v/v) it in mixed solution, is then allowed to stand in micro-wave oven, in 400W microwaves
After handling 10min, treatment fluid is obtained by filtration, mass fractions of the HCl in mixed solution is 1.5%.
(3) the treatment fluid 12000rpm of acquisition is centrifuged into 5min, gained sediment is lignin nanoparticle.
Average grain diameter by the lignin nanoparticle of the preparation of this comparative example is that (coefficient of dispersion is 534nm：
0.314).Relative to the preparation method of the comparative example, preparation method according to the present invention has following advantage：(1) present invention system
It is smaller for the lignin nanoparticle grain size gone out, there are significant nano effect, and even particle size distribution.(2) present invention is used
Concentration of hydrochloric acid it is relatively low, have economic and environment-friendly effect.
Comparative example 2
(1) 60 mesh are sieved after crushing rice straw, and ultra-pure water cleans twice, and drying to constant weight in 60 DEG C.
(2) will through step (1), treated, and rice straw is placed in counteracting tank, by solid-to-liquid ratio be 1:10 (g/ml) are added molten
Solution has the alcohol-water (ethyl alcohol of HCl：Water is 65:35, v/v) it in mixed solution, is then allowed to stand in micro-wave oven, in 400W microwaves
After handling 10min, treatment fluid is obtained by filtration, mass fractions of the HCl in mixed solution is 0.1%.
(3) the treatment fluid 12000rpm of acquisition is centrifuged into 5min, gained sediment is lignin floccule.
This comparative example can not prepare lignin nanoparticle under conditions of HCl concentration is too low.
Comparative example 3
(1) 60 mesh are sieved after crushing rice straw, and ultra-pure water cleans twice, and drying to constant weight in 60 DEG C.
(2) will through step (1), treated, and rice straw is placed in counteracting tank, by solid-to-liquid ratio be 1:10 (g/ml) are added molten
Solution has in the aqueous solution of HCl, is then allowed to stand in micro-wave oven, after 400W microwave treatments 10min, treatment fluid is obtained by filtration, institute
It is 0.5% to state mass fractions of the HCl in mixed solution.
(3) the treatment fluid 12000rpm of acquisition is centrifuged into 5min, gained sediment is lignin floccule.
This comparative example can not prepare lignin nanoparticle under conditions of solution is mixed without ethyl alcohol.
Comparative example 4
This comparative example preparation method i.e. according to the present invention and patent (application number：201710580422.4) in preparation
Method is compared.
Patent (application number：201710580422.4) in anhydrous choline chloride and lactic acid are mixed, in an oven with 60-70
DEG C temperature seal heat 2-3h, obtain homogeneous phase transparent liquid, eutectic solvent obtained after being cooled to room temperature, utilize the eutectic
Solvent is washed by filtering, absolute ethyl alcohol in sealed solvent in 90-150 DEG C of thermotonus 6-24h, obtained mixture successively
It washs, precipitate standing and obtain the lignin nanoparticle that grain size concentrates on 80-100nm after detaching.Relative in the patent
Preparation method, preparation method according to the present invention have following advantage：(1) cosolvent employed in the present invention is not required to by multiple
Miscellaneous preparation process, it is time-consuming short, and reagent is cheap, can substantially reduce industrial cost.(2) preparation method employed in the present invention
Quickly, simple and mild condition, is greatly improved industrially prepared efficiency.(3) present invention, which can synchronize, prepares a kind of granularity point
Cloth uniformly, the nitrogen-doped carbon quantum dot with notable upconversion mechanism, improve the present invention application value.
Comparative example 5
This comparative example preparation method i.e. according to the present invention and patent (application number：201410799742.5) in preparation
Method is compared.
Patent (application number：201410799742.5) in make alkali lignin be dissolved in tetrahydrofuran equal solvent using ultrasonic method
In, (100-1200rpm) is slowly equably added drop-wise in deionized water lignin liquor under high velocity agitation, most short time for adding
Control is in 1-4h, further by being centrifugally separating to obtain the lignin nanoparticle that particle diameter distribution is 100-300nm.Relative to this
Preparation method in patent, preparation method according to the present invention have following advantage：(1) equipment of the present invention is simple,
Low cost, easy realization easy to operate can substantially reduce industrial production cost, application easy to spread.(2) wood that the present invention prepares
Quality nano particle diameter is smaller, there is significant nano effect, and even particle size distribution.(3) present invention can be synchronized and be prepared
A kind of even particle size distribution, the nitrogen-doped carbon quantum dot with notable up-conversion fluorescence effect improve the application value of the present invention.
Comparative example 6
This comparative example preparation method i.e. according to the present invention and patent (application number：201610054543.0) in preparation
Method is compared.
Patent (application number：201610054543.0) in use triisopropanolamine raw material, in alcohol solvent, be added carbonization
Agent, through 100-180 DEG C, after the reaction time is 6-24h, nitrogen-doped carbon quantum dot dispersion liquid can be obtained in filtering, dialysis, then through dense
Nitrogen-doped carbon quantum dot can be obtained in contracting, freeze-drying.Relative to the preparation method in the patent, preparation side according to the present invention
Method has following advantage：(1) raw material employed in the present invention is abandoned biomass, and source is wide, at low cost, is suitble to industry metaplasia
Production, (2) the method applied in the present invention is easy to operate, and the time is short, can greatly improve preparation efficiency.(3) present invention can synchronize
Prepare a kind of even particle size distribution, the lignin nanoparticle with nanometer size effect.
Comparative example 7
This comparative example preparation method i.e. according to the present invention and patent (application number：201611105346.3) in preparation
Method is compared.
Patent (application number：201611105346.3) sisal hemp is used to carry out complicated pre-treatment first for raw material in, into one
Step is mixed in deionized water and glycerin solution, 160 DEG C, and after 200W microwave treatments 30min, filtering dialysis obtains carbon quantum
Point.Relative to the preparation method in the patent, preparation method according to the present invention has following advantage：(1) present invention is used
Lignocellulosic is not required to, by any pre-treatment, can directly be prepared, therefore, it is possible to greatly improve preparation efficiency.(2) this hair
Bright can synchronize prepares a kind of even particle size distribution, the lignin nanoparticle with nanometer size effect.
Comparative example 8
This comparative example preparation method i.e. according to the present invention and patent (application number：201510269246.3) in preparation
Method is compared.
Patent (application number：201510269246.3) after fish offal (fish scale, fish-bone and fish-skin) being cleaned, 90-200
DEG C hydro-thermal reaction, through filtering, dialysis, freeze-drying, obtains nitrogen-doped carbon quantum dot after 3-48 hours.Relative in the patent
Preparation method, preparation method according to the present invention have following advantage：(1) the method applied in the present invention is easy to operate, the time
It is short, preparation efficiency can be greatly improved, manufacturing cost is reduced.(2) present invention, which can synchronize, prepares a kind of even particle size distribution, tool
There is the lignin nanoparticle of nanometer size effect.
Claims (10)
1. a kind of method that Fast synchronization prepares lignin nanoparticle and carbon quantum dot, it is characterised in that：By abandoned biomass
It is added in acid solution, is separated by solid-liquid separation after microwave treatment and obtains treatment fluid；Treatment fluid is centrifuged, gained lower sediment is wooden
Plain nano particle, gained supernatant liquor are nitrogen-doped carbon quantum dot solution, and the solvent in the acid solution is mixed comprising ethyl alcohol
Bonding solvent；
The acid is non-oxidizing acid；
H in the acid solution+A concentration of 0.13mol/L~0.27mol/L.
2. the method that a kind of Fast synchronization according to claim 1 prepares lignin nanoparticle and carbon quantum dot, special
Sign is：The solid-liquid mass volume ratio of the abandoned biomass and acid solution is 1:10-1:20(g/ml).
3. the method that a kind of Fast synchronization according to claim 1 prepares lignin nanoparticle and carbon quantum dot, special
Sign is：The acid solution refers to the mixed solution dissolved with HCl.
4. the method that a kind of Fast synchronization according to claim 3 prepares lignin nanoparticle and carbon quantum dot, special
Sign is：Mass fractions of the HCl in acid solution is 0.5%-1%.
5. the method that a kind of Fast synchronization according to claim 4 prepares lignin nanoparticle and carbon quantum dot, special
Sign is：Mass fractions of the HCl in acid solution is 0.5%-0.8%.
6. the method that a kind of Fast synchronization according to claim 1 prepares lignin nanoparticle and carbon quantum dot, special
Sign is：The mixed solvent is made of second alcohol and water, the in the mixed solvent, and the volume ratio of second alcohol and water is 50:50-80:
20。
7. the method that a kind of Fast synchronization according to claim 6 prepares lignin nanoparticle and carbon quantum dot, special
Sign is：The volume ratio of the in the mixed solvent, second alcohol and water is 60:40-70:30.
8. the method that a kind of Fast synchronization according to claim 1 prepares lignin nanoparticle and carbon quantum dot, special
Sign is：The abandoned biomass is selected from rice straw, maize straw, wheat stalk, and at least one in bagasse, switchgrass
Kind, the mesh of the grain size of the abandoned biomass≤60.
9. the method that a kind of Fast synchronization according to claim 1 prepares lignin nanoparticle and carbon quantum dot, special
Sign is：The power of microwave treatment is 400-500W, and the time of microwave treatment is 7-15min.
10. the method that a kind of Fast synchronization according to claim 1 prepares lignin nanoparticle and carbon quantum dot, special
Sign is：The rotating speed of the centrifugation is 10000-14000rpm, time 5-10min.
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| CN110818912A (en) * | 2019-10-23 | 2020-02-21 | 广东工业大学 | Method for rapidly preparing nanoscale lignin |
| CN110857337A (en) * | 2018-08-22 | 2020-03-03 | 中南大学 | Method for synchronously preparing multiple biomass materials |
| CN113004548A (en) * | 2021-03-24 | 2021-06-22 | 中南大学 | Method for preparing lignin nanoparticles ultra-rapidly |
| CN113620274A (en) * | 2021-08-19 | 2021-11-09 | 广东工业大学 | Method for preparing lignin-based carbon quantum dots with high quantum yield quickly, simply and conveniently |
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| CN113004548B (en) * | 2021-03-24 | 2022-07-22 | 中南大学 | Method for preparing lignin nanoparticles ultra-rapidly |
| CN113620274A (en) * | 2021-08-19 | 2021-11-09 | 广东工业大学 | Method for preparing lignin-based carbon quantum dots with high quantum yield quickly, simply and conveniently |
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